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At least 595 records · Page 33Linked to original sources
PubMed2000

A REMPI method for the ultrasensitive detection of NO and NO2 using atmospheric pressure laser ionization mass spectrometry.

We report on the development of a quasi-simultaneous highly selective method for NO and NO2 detection at the ultratrace level. Atmospheric pressure laser ionization (APLI), recently introduced by our group, is used to detect both compounds at low parts per trillion by volume (pptv) mixing ratios. APLI is based on resonance-enhanced multiphoton ionization mass spectrometry. Two-color pump-probe experiments employing a single excimer pumped dye laser combination allow for the ultrasensitive measurement of NO and NO2 within a narrow range of maximum pumping efficiency of the laser dye Coumarin 120. NO is detected via excitation of the long-lived A 2sigma+ (nu' = 1) level at 215.36 nm and subsequently ionized with 308-nm radiation provided by the excimer pump laser. NO2 is ionized after double resonant excitation of the A2B1 and 3psigma manifolds in a (1 + 1' + 1(')) process using 431.65 + 308 nm. The selectivity of the NO measurement exceeds 2,000 with respect to NO2 and N2O5. For NO2, a selectivity of >3,000 with respect to N2O5 and organic nitrates is observed. The current APLI detection limit of NO and NO2 is 0.5 and 5 pptv, respectively, with a 20-s integration time.

Journal Article↗
PubMed2005

Phase-locked two-line OH planar laser-induced fluorescence thermometry in a pulsating gas turbine model combustor at atmospheric pressure.

Two-line OH planar laser-induced fluorescence (PLIF) thermometry was applied to a swirling CH4/air flame in a gas turbine (GT) model combustor at atmospheric pressure, which exhibited self-excited combustion instability. The potential and limitations of the method are discussed with respect to applications in GT-like flames. A major drawback of using OH as a temperature indicator is that no temperature information can be obtained from regions where OH radicals are missing or present in insufficient concentration. The resulting bias in the average temperature is addressed and quantified for one operating condition by a comparison with results from laser Raman measurements applied in the same flame. Care was taken to minimize saturation effects by decreasing the spectral laser power density to a minimum while keeping an acceptable spatial resolution and signal-to-noise ratio. In order to correct for the influence of laser light attenuation, absorption measurements were performed on a single-shot basis and a correction procedure was applied. The accuracy was determined to 4%-7% depending on the location within the flame and on the temperature level. A GT model combustor with an optical combustion chamber is described, and phase-locked 2D temperature distributions from a pulsating flame are presented. The temperature variations during an oscillation cycle are specified, and the general flame behavior is described. Our main goals are the evaluation of the OH PLIF thermometry and the characterization of a pulsating GT-like flame.

Journal Article↗
PubMed1997

Identification of ceramides in human cells using liquid chromatography with detection by atmospheric pressure chemical ionization-mass spectrometry.

Ceramides are intermediates in the biosynthesis of membrane sphingolipids. These biomolecules are also important as second messengers in signal transduction pathways controlling cell growth. We have developed two reversed-phase high pressure liquid chromatography (RPHPLC) techniques for identification and quantification of ceramides from mammalian cells. One method was based on atmospheric pressure chemical ionization-mass spectrometry (APCI-MS) detection of ceramides and had the advantage of requiring minimal sample preparation, yielding significant structural information, and affording high sensitivity. The second method relied on perbenzoylation of the ceramides and detection at 230 nm. The predominant ceramides detected in the human leukemic HL-60 cell were N-(palmitoyl)-sphingosine, N-(nervonyl)-sphingosine, and N-(lignoceroyl)-sphingosine. When selected ion monitoring was used with RPHPLC/APCI-MS, approximately 2.2 pmol N-(palmitoyl)-sphingosine and 1.7 pmol N-(nervonyl)-sphingosine were observed in an extract from 40,000 HL-60 cells. Perbenzoylation with benzoyl chloride permitted RPHPLC separation and 230 nm UV absorbance detection of the trisbenzoyl derivatives of sphingosine, N-(palmitoyl)-sphingosine, N-(nervonyl)-sphingosine, and N-(lignoceroyl)-sphingosine in the HL-60 cells. These results demonstrate the utility of utilizing two different methods coupled with APCI-MS for the quantification and identification of ceramides in biological samples.

Benzyl Compounds↗
PubMed1992

Screening of organophosphorus pesticides using liquid chromatography-atmospheric pressure chemical ionization mass spectrometry.

Screening and identification of organophosphorus pesticides in blood from patients suffering from acute agricultural chemical toxicity were established by a liquid chromatography-atmospheric pressure chemical ionization mass spectrometric method. To determine 21 pesticides, it was necessary to monitor both positive and negative ions. This method could easily screen for 21 organophosphorus pesticides in less than 30 min. By comparison with a gas chromatographic-mass spectrometric method, the chemicals indicated a similar extent of specificity and within equivalent detection limits, thus satisfying clinical requirements completely.

Chromatography↗
PubMed2000

Determination of pesticides in soil samples by supercritical fluid chromatography-atmospheric pressure chemical ionisation mass spectrometric detection.

This paper presents an analytical technique for the determination of pesticides in soil by packed-column supercritical fluid chromatography interfaced with atmospheric pressure chemical ionisation mass spectrometry (pSFC-APCI-MS). The technique provides a versatile method for the detection and quantification of pesticides belonging to three different commonly used classes, triazines (ametryne, atrazine), carbamates (carbofuran) and sulfonylureas (chlorsulfuron, metsulfuron methyl and benzsulfuron methyl). The APCI mass spectra for all the pesticides studied consisted of protonated molecule ions as the most abundant ion at low cone voltages, except for metsulfuron methyl and benzsulfuron methyl, which gave a fragment ion as the most abundant ion with the protonated molecule ion at low intensity. Increasing the cone voltage provided informative fragmentation patterns for all species. The technique shows good linearity over the concentration range of 0.1-50 micrograms ml-1, with r2 values as follows: atrazine 0.997, ametryne 0.995, carbofuran 0.999, benzsulfuron methyl 0.999, chlorsulfuron 0.995 and metsulfuron methyl 0.997. The detection limits in the selected ion mode were atrazine 201, ametryne 144 and carbofuran 385 pg, which were calculated by using the standard solution, and benzsulfuron methyl 2.045, chlorsulfuron 1.435 and metsulfuron methyl 2.414 ng, which were determined by using spiked soil samples. The pSFC-MS system was shown to have a high degree of reproducibility. The technique was then applied to the determination of the above pesticides in soil samples. The results obtained show that there is no matrix effect from the soil and that the detection limits for all pesticides in soil were similar to those found for the standard solutions.

Chromatography, Ion Exchange↗
PubMed2004

Determination of polycyclic aromatic hydrocarbons in sediment by liquid chromatography-atmospheric pressure photoionization-mass spectrometry.

We describe a method for the simultaneous determination of 12 kinds of polycyclic aromatic hydrocarbons (PAHs) in sediment based on liquid chromatography-atmospheric pressure photoionization-mass spectrometry (LC/APPI/MS). The method consists of PAH extractions by ultrasonics, clean-up by a solid-phase extraction procedure and determination by LC/APPI/MS. The limits of the determination for PAHs in sediment using the proposed method ranged from 0.06 to 0.9 mg/kg. PAHs were detected by this method in sediment samples on the mg/kg level.

Journal Article↗
PubMed2003

Is the atmospheric pressure chemical ionisation and collisionally induced methanol loss from protonated dehydroamino acids a retrosynthetic process?

Unsaturated 5(4H)-oxazolones lead, by methanolysis, to the corresponding dehydroamino acid derivatives. Interestingly, under atmospheric pressure chemical ionisation (APCI) conditions, the latter give rise, aside from abundant [M+H](+) ions, to [MHbondCH(3)OH](+) species, formally corresponding to the protonated oxazolones employed for their synthesis. Retrosynthetic processes have often been described as energetically favoured decompositions of odd-electron molecular ions but never invoked in APCI-activated fragmentations. To investigate this possible retrosynthetic process, occurring also under collisional conditions, some experiments on the deuterated analogues have been undertaken. The breakdown curves of [M+H](+) of oxazolones and [MHbondCH(3)OH](+) of the dehydroamino acid derivatives are superimposable, proving their structural identity and giving experimental evidence of the occurrence of a real retrosynthetic process from even-electron protonated molecules.

Journal Article↗
PubMed1993

Simple, rapid and simultaneous measurement of eight different types of carbamate pesticides in serum using liquid chromatography-atmospheric pressure chemical ionization mass spectrometry.

We have developed a method for simultaneous analysis of methylcarbamate pesticides in serum with an acute pesticide intoxication. This is performed by liquid chromatography-atmospheric pressure chemical ionization mass spectrometry. Rapid detection of eight types of methylcarbamate pesticide can be achieved with this method, it only requires an extremely simple pre-treatment of the sample. The specificity of this method is equal to that of gas chromatography-mass spectrometry, and it satisfies the clinical requirements for detection sensitivity and specificity. Although some problems with this analytical method remain to be solved, we consider it to be superior to any other analytical method previously reported.

Acetates↗
PubMed1997

Liquid chromatography-atmospheric-pressure chemical ionization mass spectrometry as a routine method for the analysis of mutagenic amines in beef extracts.

A liquid chromatography-mass spectrometry (LC-MS) method using atmospheric-pressure chemical ionisation as interface was developed for the simultaneous determination of 14 heterocyclic aromatic amines and related compounds in beef extracts. The separation was performed on a conventional C18 column using a binary mobile phase composed of acetonitrile and 50 mM ammonium acetate at pH 5.7, and elution was carried out in gradient mode. Several parameters influencing the mass spectra were optimized, and the effect of the variation of cone voltage on the mass spectra was studied. The [M+H]+ ions and some fragments produced in the source were observed in the mass spectra when several extraction voltages were applied. Quality parameters (run-to-run and day-to-day reproducibility, intervals of linearity, and limits of detection) were studied in the optimum working conditions. The method was used to analyze the heterocyclic amines present in a commercial beef extract. Therefore, a solid-phase extraction clean-up procedure was performed prior the LC-MS analysis due to the complexity of the sample and the compounds Glu-P-1, Harman, Norharman and A alpha C were identified in the samples at ppb levels and successfully confirmed using in-source fragmentation.

Amines↗
PubMed1997

Rapid target analysis of microcontaminants in water by on-line single-short-column liquid chromatography combined with atmospheric pressure chemical ionization tandem mass spectrometry.

The applicability of trace enrichment and separation of microcontaminants on a 10 mm x 2 mm I.D. high-pressure packed (8 microns C18 bonded silica or 10-15 microns PLRP-S) column combined on-line with an atmospheric pressure chemical ionization MS-MS system is demonstrated for the target analysis of herbicides in river water. Tailor-made procedures are obtained for a limited number of analytes by tuning the chromatographic efficiency of the short LC column and the specificity of tandem MS, in order to minimize the analysis time. With the on-line short-column LC-MS-MS method, good linearity is obtained for the herbicides in the range of 0.1-10 micrograms/l. The relative standard deviations of peak areas are less than 5% and, with only 4-ml samples, detection limits of 0.01-0.1 microgram/l can be achieved. The total analysis time is 10-15 min. The 10 mm x 2 mm I.D. LC columns packed with 8 microns particles show good stability and can be used for at least 40 analyses. Target compound analyses of river water allowed the confirmation of the presence of herbicides such as diuron, simazine, atrazine and terbutylazine at sub-microgram/l levels.

Chromatography, High Pressure Liquid↗
PubMed2000

Electrospray and atmospheric pressure chemical ionization tandem mass spectrometric behavior of eight anabolic steroid glucuronides.

Mass spectrometric and tandem mass spectrometric behavior of eight anabolic steroid glucuronides were examined using electrospray (ESI) and atmospheric pressure chemical ionization (APCI) in negative and positive ion mode. The objective was to elucidate the most suitable ionization method to produce intense structure specific product ions and to examine the possibilities of distinguishing between isomeric steroid glucuronides. The analytes were glucuronide conjugates of testosterone (TG), epitestosterone (ETG), nandrolone (NG), androsterone (AG), 5alpha-estran-3alpha-ol-17-one (5alpha-NG), 5beta-estran-3alpha-ol-17-one (5beta-NG), 17alpha-methyl-5alpha-androstane-3alpha,17beta-diol (5alpha-MTG), and 17alpha-methyl-5beta-androstane-3alpha,17beta-diol (5beta-MTG), the last four being new compounds synthesized with enzyme-assisted method in our laboratory. High proton affinity of the 4-ene-3-one system in the steroid structure favored the formation of protonated molecule [M + H]+ in positive ion mode mass spectrometry (MS), whereas the steroid glucuronides with lower proton affinities were detected mainly as ammonium adducts [M + NH4]+. The only ion produced in negative ion mode mass spectrometry was a very intense and stable deprotonated molecule [M - H]- . Positive ion ESI and APCI MS/MS spectra showed abundant and structure specific product ions [M + H - Glu]+, [M + H - Glu - H2O]+, and [M + H - Glu - 2H2O]+ of protonated molecules and corresponding ions of the ammonium adduct ions. The ratio of the relative abundances of these ions and the stability of the precursor ion provided distinction of 5alpha-NG and 5beta-NG isomers and TG and ETG isomers. Corresponding diagnostic ions were only minor peaks in negative ion MS/MS spectra. It was shown that positive ion ESI MS/MS is the most promising method for further development of LC-MS methods for anabolic steroid glucuronides.

Anabolic Agents↗
PubMed2002

[Temporal behavior of light emission of dielectric barrier discharges in air at atmospheric pressure].

The experimental setup of dielectric barrier discharge was designed which is propitious to optical measurement. Temporal behavior of light emission of dielectric barrier discharges (filamentary model) in air at atmospheric pressure was measured by using optical method. Temporal behavior of dielectric barrier discharges was obtained. The experimental results show that the discharge burst in each half cycle of applied voltage consists of a series of discharge pulses, the duration of each discharge pulse is about 30-50 ns, and the interval of the neighboring discharge pulses is about a few hundred ns. The result is of great importance to the application of dielectric barrier discharges.

English Abstract↗
PubMed2001

Structural assignment of isomeric 2-(2-quinolinyl)-1H-indene-1,3(2H)-dione mono- and disulfonic acids by liquid chromatography electrospray and atmospheric pressure chemical ionization tandem mass spectrometry.

Positionally isomeric 2-(2-quinolinyl)-1H-indene-1,3(2H)-dione mono- and disulfonic acids give rise to similar electrospray ionization (ESI) and atmosphere pressure chemical ionization (APCI) mass spectra, which show very abundant MH(+) ions and negligible fragmentation. The MH(+) ions of these isomeric acids exhibit notably different behavior under collision-induced dissociation (CID) conditions. The acids with a sulfonic group at position 8' in the quinoline moiety, adjacent to the N-atom, exhibit highly abundant [MH - H(2)SO(3)](+) ions (m/z 272 for the mono- and m/z 352 for the disulfonic acids), which are of lower abundance in the CID spectra of isomers with the SO(3)H group at other positions, remote from the nitrogen atom. The latter isomers undergo efficient eliminations of SO(3) and HSO(3). The isomeric diacids with one SO(3)H group at position 4 of the indene-1,3(2H)-dione moiety, adjacent to one of the carbonyl groups, undergo highly efficient elimination of H(2)O. Mechanistic pathways, involving interactions between adjacent groups, are proposed for the above regiospecific fragmentations. Pronounced different behavior has been also observed in negative ion tandem mass spectrometric measurements of the sulfonic acids. The distinctive behavior of the isomeric acids was strongly pronounced when the measurements were performed with an ion trap mass spectrometer (LCQ), and much less so with a triple-stage quadrupole instrument (TSQ).

Coloring Agents↗
PubMed2001

Fast confirmation of 11-nor-9-carboxy-Delta(9)-tetrahydrocannabinol (THC-COOH) in urine by LC/MS/MS using negative atmospheric-pressure chemical ionisation (APCI).

A fast method using automated solid-phase extraction (SPE) and short-column liquid-chromatography coupled to tandem mass-spectrometry (LC/MS/MS) with negative atmospheric-pressure chemical ionisation (APCI) has been developed for the confirmation of 11-nor-9-carboxy-Delta(9)-tetrahydrocannabinol (THC-COOH) in urine samples. This highly specific method which combines chromatographic separation and MS/MS-analysis can be used for the confirmation of positive immunoassay results with a NIDA cut-off of 15ng/ml. The conjugates of THC-COOH were hydrolysed prior to SPE, and a standard SPE was performed using C18-SPE columns. No derivatisation of the extracts was needed as in GC/MS analysis, and the LC run-time was 6.5min by gradient elution with a retention time of 2.4min. Linearity of calibration was obtained in the range between 0 and 500ng/ml (correlation coefficient R(2)=0.998). Using linear regression (0-50ng/ml) the limit of detection (LOD) was 2.0ng/ml and the limit of quantitation (LOQ) was 5.1ng/ml; day-to-day reproducibility and precision were tested at 15 and 250ng/ml and were 13.4ng/ml+/-3.3% and 255.8ng/ml+/-4.5%, respectively.

Chromatography, Liquid↗
PubMed2001

Analysis of organophosphorus pesticides in honeybee by liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry.

Pesticides applied in extended agricultural fields may be controlled by means of bioindicators, such as honeybees, in which are the pesticides bioaccumulate. Liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) experiments with positive (PI) and negative (NI) ion modes were optimized for the analysis of 22 organophosphorus pesticides in honeybee samples. The extraction required 3 g of sample, which was extracted with acetone. The extract was purified with coagulating solution and reextracted with Cl(2)CH(2). Pesticides studied could be detected by both ionization modes except for parathion, parathion-methyl, and bromophos, which did not give signals in PI mode, and triazophos, which was not detected in NI mode. Fragmentation voltage and vaporizer temperature were optimized to achieve the highest sensitivity. The spectra profile of each pesticide in PI mode showed the [M + H](+) ion as the main signal, whereas in NI mode only fragment ions were shown. The detection limit obtained in selected ion monitoring mode ranged from 1 to 15 microg kg(-1). The average recoveries from spiked honeybees at various concentration levels (0.5-5 mg kg(-1)) exceeded 65% with relative standard deviations of 4-15%. The method was applied to real samples, in which residues of coumaphos and dimethoate were detected.

Animals↗
PubMed2005

Observation of spiral pattern and spiral defect chaos in dielectric barrier discharge in argon/air at atmospheric pressure.

A rich variety of spiral patterns such as single-armed spiral, dipole spirals, target pattern, multiarmed spiral, and spiral defect chaos state have been observed in ac-driven atmospheric pressure gas discharge. The confined and free boundary conditions are defined by means of whether there is a sidewall in the discharge domain or not, respectively. In the free boundary condition, the spiral pattern arises when the stripe pattern undergoes core instability or notching instability. In the confined boundary condition, the spiral pattern is formed by sidewall forcing. The spiral drifts upward in the free boundary condition and meanders in the confined boundary condition. The topological charge of the spiral pattern can be changed when the spiral interacts with the dislocations. The spiral wavelength (average distance between two consecutive rolls) is a function of gas composition and decreases rapidly with increase of air concentration in discharge gas.

Journal Article↗
PubMed1999

Application of liquid chromatography atmospheric pressure chemical ionization tandem mass spectrometry in the quantitative analysis of glyburide (glibenclamide) in human plasma.

Glyburide (glibenclamide) is widely prescribed in the treatment of Type II diabetes. A validated liquid chromatography atmospheric pressure chemical ionization tandem mass spectrometry (LC/APCI-MS/MS) method for the determination of glyburide is reported. The method uses a stable isotope labeled glyburide as the internal standard. Subsequent to acetonitrile protein precipitation, the supernatant was directly (unfiltered) injected onto the LC column (retention time approximately 3 min) for analysis. A lower limit of quantification (LLOQ) of 1.01 ng/mL was attained for the human plasma assay. The method was fast, specific, and exhibited excellent ruggedness. It was successfully applied to the analysis of clinical samples from patients dosed with glyburide.

Calibration↗